CN102631440A - External traditional Chinese medicine preparation for treating burns and scalds as well as preparation method and quality detection method of preparation - Google Patents
External traditional Chinese medicine preparation for treating burns and scalds as well as preparation method and quality detection method of preparation Download PDFInfo
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Abstract
The invention belongs to the field of traditional Chinese medicine preparation, relates to an external traditional Chinese medicine preparation for treating burns and scalds as well as the preparation method and the quality detection method of the preparation, and in particular relates to a preparation method and a quality detection method of a linimentum for burns and scalds. According to the invention, a new quality control method of a linimentum for burns and scalds is established. The quality detection method comprises the following steps: identifying rhubarb, borneol and lithospermum in the linimentum by adopting thin layer chromatography; and carrying out content determination of camphol in the borneol by using high performance liquid chromatography. The quality detection method has the following advantage that (1) the quality control method is comprehensive and simple and has good accuracy, sensitivity and stability to ensure stable and controllable product quality; and (2) the comprehensive quality detection method of the linimentum for burns and scalds is established to comprehensively detect preparation quality and ensure the safety and effect of clinical medication.
Description
Technical field
The invention belongs to field of traditional Chinese, relate to a kind of Chinese medicine for external application of treating burn and scald and preparation thereof, quality determining method, be specifically related to the preparation and the quality determining method of burn and scald liniment.
Background technology
The burn and scald liniment is a kind of compound Chinese medicinal preparation of having gone on the market, and has clearing away heat to alleviate pain, the effect of removing heat from blood putrefaction removing.Be mainly used in the treatment that I, II degree burn and scald and soda acid are burnt clinically; But existing burn and scald standard preparation detects the index imperfection, and the quality determining method of prior art can not be controlled the quality of burn and scald liniment comprehensively, thereby will influence the quality of production control and the drug safety of product.
Summary of the invention
The purpose of this invention is to provide a kind of Chinese medicine for external application of treating burn and scald and preparation thereof, quality determining method; Particularly provide a kind of quality determining method to make it can control the quality of burn and scald liniment comprehensively, thereby guarantee the quality of production and the drug safety of product.
A kind of Chinese medicine for external application of treating burn and scald of the present invention, formulated by following crude drug: Radix et Rhizoma Thalictri 85～102g, Radix Arnebiae (Radix Lithospermi) 56～69g, Radix Scutellariae 85～102g, Radix Sanguisorbae 56～69g, Radix Et Rhizoma Rhei 56～69g and Borneolum Syntheticum 4～6g.
Wherein, optimal technical scheme is following: formulated by following crude drug: Radix et Rhizoma Thalictri 93g, Radix Arnebiae (Radix Lithospermi) 62.4g, Radix Scutellariae 93g, Radix Sanguisorbae 62.4g, Radix Et Rhizoma Rhei 62.4g and Borneolum Syntheticum 5g.
The method for preparing of the Chinese medicine for external application of treatment burn and scald of the present invention, it is fried to withered and yellow after 18～36 hours with the Oleum sesami immersion of 1170～1430g to get Radix et Rhizoma Thalictri, Radix Et Rhizoma Rhei, Radix Arnebiae (Radix Lithospermi), Radix Sanguisorbae and Radix Scutellariae, filters; The Cera Flava that adds 15～25g immediately when temperature is reduced to 55～65 ℃, adds Borneolum Syntheticum; Stirring makes its dissolving, when reducing to room temperature, adds the phenol of 4～5ml; Stir, fill promptly gets.
The quality determining method of the Chinese medicine for external application of treatment burn and scald of the present invention comprises the quality testing of following aspect:
(1) thin layer of Radix Et Rhizoma Rhei is differentiated:
Get the Chinese medicine for external application 10ml of treatment burn and scald, with alcohol extraction 3 times, each 10ml, merging ethanol liquid is put evaporate to dryness in the water-bath, and residue adds ethanol 1ml makes its dissolving, as need testing solution; Other gets the chrysophanol reference substance, adds ethyl acetate and processes the solution that every 1ml contains 1mg, as reference substance solution;
According to the check of an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 5～10 μ l, reference substance solution 2～5 μ l; Put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be that 15: 5: 1 petroleum ether, Ethyl formate and formic acid mixtures is developing solvent with volume ratio, launch; Take out, dry, under the ultra-violet lamp of 365nm, inspect; Wherein, the boiling point of petroleum ether is 30～60 ℃;
The thin layer of Radix Et Rhizoma Rhei differentiates that criterion of acceptability is: in the test sample chromatograph with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(2) thin layer of Borneolum Syntheticum is differentiated:
Get the Chinese medicine for external application 10ml of treatment burn and scald, with alcohol extraction 3 times, each 10ml, merging ethanol liquid is put evaporate to dryness in the water-bath, and residue adds ethanol 1ml makes its dissolving, as need testing solution; Other gets the Borneolum Syntheticum reference substance, adds ethanol and processes the solution that every 1ml contains 5mg, as reference substance solution;
According to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography check, draw need testing solution 10 μ l, reference substance solution 2～5 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose; With volume ratio is that 9: 1 petroleum ether and ethyl acetate mixture is developing solvent, launches, and takes out; Dry, spray is with 1wt% vanillin sulfuric acid solution, and hot blast drying to clear spot is inspected; Wherein, the boiling point of petroleum ether is 60～90 ℃;
The thin layer of Borneolum Syntheticum differentiates that criterion of acceptability is: in the test sample chromatograph with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(3) thin layer of Radix Arnebiae (Radix Lithospermi) is differentiated:
Get the Chinese medicine for external application 20ml of treatment burn and scald, with ethanol extraction 3 times, each 20ml, merging ethanol liquid evaporate to dryness, residue adds ethanol 1ml makes its dissolving, as need testing solution; Other gets Radix Arnebiae (Radix Lithospermi) control medicinal material lg, adds ethanol 10ml dipping 2 hours, filters, and gets filtrating 1ml as reference substance solution;
Check according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography; Draw need testing solution 10 μ l, reference substance solution 2～5 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be 5: 5: 0.5 with volume ratio: 0.1 cyclohexane extraction, toluene, ethyl acetate and formic acid mixtures are developing solvent; Launch; Take out, dry, inspect;
The thin layer of Radix Arnebiae (Radix Lithospermi) differentiates that criterion of acceptability is: in the test sample chromatograph with the corresponding position of reference substance chromatograph on, show the speckle of same color, spray is with behind 10% potassium hydroxide methanol solution, speckle becomes blueness.
(4) assay of Borneolum Syntheticum in the Borneolum Syntheticum:
Chromatographic condition and system suitability test: the Rtx-Wax capillary column of 30m * 0.53mm * 1.00 μ m, Polyethylene Glycol PEG-20M is an immobile phase; Flame ionization ditector; Injection port, detector temperature are 210 ℃; 150 ℃ of column temperatures; Post flow 8ml/min; Split sampling, split ratio 9: 1; Theoretical cam curve is calculated by the Borneolum Syntheticum peak should be not less than 6000;
The preparation of inner mark solution: it is an amount of that precision takes by weighing the methyl salicylate reference substance, adds ethyl acetate and process the solution that every 1ml contains 0.8mg, subsequent use;
The preparation of reference substance solution: precision takes by weighing the Borneolum Syntheticum reference substance, adds inner mark solution 1ml, is settled to 10ml with ethyl acetate, processes the solution that every 1ml contains 0.05mg, and is subsequent use;
The preparation of need testing solution: get the Chinese medicine for external application 0.5g of treatment burn and scald, the accurate title, decide, and puts in the 10ml volumetric flask, adds inner mark solution 1ml, is settled to 10ml with ethyl acetate, and mixing filters with 0.45 μ m microporous filter membrane, and is subsequent use;
Algoscopy: accurate respectively reference substance solution and each 1 μ l of need testing solution of drawing, inject gas chromatograph is measured, and promptly gets.
The detection criterion of acceptability of the content of Borneolum Syntheticum is in the Borneolum Syntheticum: these article contain Borneolum Syntheticum in Borneolum Syntheticum, must not be less than 0.9mg/g.
The invention has the advantages that: (1) this method of quality control is comprehensive, and precision, sensitivity, stability are all good, and method is simpler and more direct, can guarantee that constant product quality is controlled; (2) set up the comprehensive quality determining method of burn and scald liniment, the ability complete detection quality of the pharmaceutical preparations guarantees that clinical drug safety is effective.
Description of drawings
Fig. 1 is that the thin layer of embodiment 1 Radix Et Rhizoma Rhei is differentiated collection of illustrative plates, and among the figure, 1,2,3 is need testing solution 4, reference substance solution 5, negative solution;
Fig. 2 is that the thin layer of embodiment 1 Borneolum Syntheticum is differentiated collection of illustrative plates, and among the figure, 1,2,3 is need testing solution 4, reference substance solution 5, negative solution;
Fig. 3 is that the thin layer of embodiment 1 Radix Arnebiae (Radix Lithospermi) is differentiated collection of illustrative plates A, and among the figure, 1,2,3 is need testing solution 4, reference substance solution 5, negative solution;
Fig. 4 is that the thin layer of embodiment 1 Radix Arnebiae (Radix Lithospermi) is differentiated collection of illustrative plates B; Among the figure, 1,2,3 is need testing solution 4, reference substance solution 5, negative solution;
Fig. 5 is the omnidistance high-efficient liquid phase chromatogram of the Borneolum Syntheticum reference substance solution of negative control test among the embodiment 1;
Fig. 6 is the omnidistance high-efficient liquid phase chromatogram of the Borneolum Syntheticum medical material solution of negative control test among the embodiment 1;
Fig. 7 is the omnidistance high-efficient liquid phase chromatogram of the negative controls of negative control test among the embodiment 1;
Fig. 8 is the omnidistance high-efficient liquid phase chromatogram of the burn and scald need testing solution of negative control test among the embodiment 1;
Fig. 9 is the standard curve of Borneolum Syntheticum.
The specific embodiment
Below in conjunction with embodiment the present invention is further specified.
Embodiment 1:
Prescription: Radix et Rhizoma Thalictri 93g, Radix Arnebiae (Radix Lithospermi) 62.4g, Radix Scutellariae 93g, Radix Sanguisorbae 62.4g, Radix Et Rhizoma Rhei 62.4g and Borneolum Syntheticum 5g.
Method for preparing: it is fried to withered and yellow after 24 hours with the Oleum sesami immersion of 1300g to get Radix et Rhizoma Thalictri, Radix Et Rhizoma Rhei, Radix Arnebiae (Radix Lithospermi), Radix Sanguisorbae and Radix Scutellariae, filters, and adds the Cera Flava of 20g immediately; When temperature is reduced to 60 ℃, add Borneolum Syntheticum, stir and make its dissolving; When reducing to room temperature; Add the phenol of 4.5ml, stir, fill promptly gets.
Obtain 060301,060302,060,303 3 batch of medicine of Rongchang Pharmaceutical (Zibo) Co., Ltd. according to above-mentioned requirements, and be used as following quality testing respectively with this.
(1) thin layer of Radix Et Rhizoma Rhei is differentiated:
The preparation of need testing solution: the article 10ml that gets it filled, with alcohol extraction 3 times, each 10ml merges ethanol liquid, puts evaporate to dryness in the water-bath, and residue adds ethanol 1ml makes dissolving, as need testing solution, in this way, prepares 3 batches of need testing solutions.
The preparation of reference substance solution: get the chrysophanol reference substance, add ethyl acetate and process the solution that every 1ml contains 1mg, as reference substance solution.
The preparation of negative solution: the Radix Et Rhizoma Rhei in will filling a prescription is removed, and other five tastes prepare the negative control sample by the method for making item in the quality standard; Method for preparing according to need testing solution prepares with method then.
Lamellae: homemade is the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, and specification is 10 * 20cm, and coating thickness is 0.3mm.
Point sample: special-purpose quantitatively capillary tube contact round point shape point sample, the point sample amount is need testing solution 10 μ l, reference substance solution 5 μ l.The point sample amount 10 μ l of negative solution.
Developing solvent: petroleum ether (30～60 ℃)-Ethyl formate-formic acid (mass ratio 15: 5: 1).
Expansion mode: the double flute expansion cylinder, ascending development, the exhibition distance is 10cm.
The colour developing with inspect: inspect under the ultra-violet lamp (365nm)
The result: in the test sample chromatograph with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color, negative noiseless.The chromatogram result of three lot sample article sees Fig. 1.
(2) thin layer of Borneolum Syntheticum is differentiated:
The preparation of need testing solution: the article 10ml that gets it filled, with alcohol extraction 3 times, each 10ml merges ethanol liquid, puts evaporate to dryness in the water-bath, and residue adds ethanol 1ml makes dissolving, as need testing solution.In this way, 3 batches of need testing solutions of preparation.The preparation of reference substance solution: get the Borneolum Syntheticum reference substance, add ethanol and process the solution that every 1ml contains 5mg, as reference substance solution.
The preparation of negative solution: the Borneolum Syntheticum in will filling a prescription is removed, and other five tastes prepare the negative control sample by the method for making item in the quality standard; Method for preparing according to need testing solution prepares with method then.
Lamellae: homemade is the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, and specification is 10 * 20cm, and coating thickness is 0.3mm.
Point sample: special-purpose quantitatively capillary tube contact round point shape point sample, the point sample amount is need testing solution 10 μ l, reference substance solution 5 μ l.The point sample amount 10 μ l of negative solution.
Developing solvent: petroleum ether (60～90 ℃)-ethyl acetate (mass ratio 9: 1).
Expansion mode: the double flute expansion cylinder, ascending development, the exhibition distance is 10-12cm.
The colour developing with inspect: the spray with 1% vanillin sulfuric acid solution, hot blast drying is to clear spot.
The result: in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color, negative control is noiseless.The result of three lot sample article sees accompanying drawing 2.
(3) thin layer of Radix Arnebiae (Radix Lithospermi) is differentiated:
The preparation of need testing solution: get scald oil 20ml, with ethanol extraction 3 times, each 20ml merges ethanol liquid evaporate to dryness, and residue adds ethanol 1ml makes dissolving, as need testing solution.In this way, 3 batches of need testing solutions of preparation.
The preparation of control medicinal material solution: get Radix Arnebiae (Radix Lithospermi) control medicinal material 1g, add ethanol 10ml dipping 2 hours, filter, get filtrating 1ml as control medicinal material solution.
The preparation of negative solution: the Radix Arnebiae (Radix Lithospermi) in will filling a prescription is removed, and other five tastes prepare the negative control sample by the method for making item in the quality standard; Method for preparing according to need testing solution prepares with method then.
Lamellae: homemade is the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, and specification is 10 * 20cm, and coating thickness is 0.3mm.
Point sample: special-purpose quantitatively capillary tube contact round point shape point sample, the point sample amount is need testing solution 10 μ l, reference substance solution 5 μ l.The point sample amount 10 μ l of negative solution.
Developing solvent: cyclohexane extraction-toluene-ethyl acetate-formic acid (mass ratio 5: 5: 0.5: 0.1).
Expansion mode: the double flute expansion cylinder, ascending development, the exhibition distance is 10-12cm.
The colour developing with inspect: the spray with behind 10% potassium hydroxide methanol solution, speckle becomes blueness.
The result: in the test sample chromatograph with the corresponding position of reference substance chromatograph on, show the speckle of same color, spray is with behind 10% potassium hydroxide methanol solution, speckle becomes blueness, negative control is noiseless.The result of three lot sample article sees Fig. 3, Fig. 4.
(4) assay of Borneolum Syntheticum in the Borneolum Syntheticum:
1) instrument and reagent
Instrument: day island proper Tianjin GC-2014 gas chromatograph; Capillary column Rtx-Wax (30m * 0.53mm * 1.00 μ m); Polyethylene Glycol PEG-20M is an immobile phase, flame ionization ditector (FID), Gcsolution data processing software; Startorius BP211D electronic analytical balance d=0.01mg, startorius BS124S electronic analytical balance d=0.1mg.
Reagent: water is redistilled water, and all the other reagent are analytical pure.
Borneolum Syntheticum reference substance (Nat'l Pharmaceutical & Biological Products Control Institute supplies assay to use for 110881-200504,20mg).
Methyl salicylate reference substance (Nat'l Pharmaceutical & Biological Products Control Institute supplies assay to use for 707-200106,1ml).
2) selection of chromatographic condition
Adopt day island proper Tianjin GC-2014 gas chromatograph, split sampling, split ratio 9: 1, injection port, detector temperature are 210 ℃, sample size 1 μ l.Consider that column temperature and post flow are bigger to the chromatographic peak influence, so the gentle post flow of coupled columns has carried out test and Selection.
3) preparation of reference substance, need testing solution
Inner mark solution: it is an amount of that precision takes by weighing the methyl salicylate reference substance, adds ethyl acetate and process the solution that every 1ml contains 0.8mg, promptly gets.
Reference substance solution: it is an amount of that precision takes by weighing the Borneolum Syntheticum reference substance, adds inner mark solution 1ml, is settled to 10ml with ethyl acetate, processes the solution that every 1ml contains 0.05mg, promptly gets.
Need testing solution: get 060302 crowd crowd of these article 0.5g under the content uniformity item, the accurate title, decide, and puts in the 10ml volumetric flask, adds inner mark solution 1ml, is settled to 10ml with ethyl acetate, and mixing filters with 0.45 μ m microporous filter membrane, promptly gets.
4) column temperature is selected
Column temperature is made as 130 ℃, 140 ℃, 150 ℃, 160 ℃ respectively; Same reference substance and burn and scald need testing solution are tested, and Borneolum Syntheticum peak and methyl salicylate peak-to-peak shape were good when column temperature was 150 ℃ as a result, and separating degree is all greater than 2.0; And appearance time is shorter, so confirm that column temperature is 150 ℃.
5) the post flow is selected:
The post flow is made as 6ml/min, 8ml/min, 10ml/min respectively; Same reference substance and burn and scald need testing solution are tested; Borneolum Syntheticum peak and methyl salicylate peak-to-peak shape were good when the post flow was 8ml/min as a result, and separating degree is all greater than 1.5, and appearance time is shorter; Than post flow is that 10ml/min saves carrier gas, so confirm that the post flow is 8ml/min.
6) negative control test:
Get the burn and scald negative sample 0.5g that does not contain Borneolum Syntheticum; Borneolum Syntheticum medical material fine powder 5mg after the same method is handled, makes negative controls and Borneolum Syntheticum medical material solution respectively; Get reference substance solution, Borneolum Syntheticum medical material solution, negative controls, each 1 μ l inject gas chromatograph of burn and scald need testing solution respectively; The record chromatogram can be found out that by Fig. 5～Fig. 8 the Borneolum Syntheticum peak is noiseless in the negative control collection of illustrative plates.
6) precision test:
The accurate Borneolum Syntheticum reference substance solution (Borneolum Syntheticum 0.070mg/ml, interior mark 0.0735mg/ml) of drawing repeats sample introduction 6 times, each each 1 μ l, and the record peak area also calculates f value and RSD, and the result sees table 1.
Table 1: Precision test result
The result shows: the RSD of f value is 0.51%, proves that this method elaboration is good.
6) range of linearity is investigated:
It is an amount of that precision takes by weighing the Borneolum Syntheticum reference substance, adds the reference substance solution that inner mark solution is processed (containing methyl salicylate 0.077mg/ml) 0.34mg/ml.The accurate 1ml reference substance solution of drawing is diluted to 2ml with above-mentioned inner mark solution, successively gradient dilution; Respectively getting 1 μ l inject gas chromatograph measures.With Borneolum Syntheticum concentration is abscissa, and the ratio of Borneolum Syntheticum peak area and interior mark peak area is vertical coordinate drawing standard curve, calculates regression equation y=19.831x-0.0525, and correlation coefficient r=0.9998 is as shown in Figure 9.Show that Borneolum Syntheticum concentration is good in 0.022～0.340mg/ml scope internal linear relation.
Table 2: the range of linearity is investigated result (n=2)
| Borneolum Syntheticum peak area/interior mark peak area | 6.7319 | 3.2209 | 1.6450 | 0.8176 | 0.4102 |
| Borneolum Syntheticum concentration (mg/ml) | 0.340 | 0.170 | 0.085 | 0.043 | 0.022 |
7) stability test:
Get 060302 batch with a need testing solution, respectively at 0 hour, 2 hours, 4 hours, 6 hours, 8 hours sample introductions, the record result also calculated the Borneolum Syntheticum peak and the methyl salicylate peak area ratio.The result sees table 3.
Table 3: sample stability result of the test (n=1)
The result shows: test sample Borneolum Syntheticum peak and methyl salicylate peak area ratio RSD in 8 hours are 1.57%, and need testing solution is good at 8 hours internal stabilities.
8) repeatability test:
Get 5 parts of 060302 lot sample article, press a test sample preparation below method preparation respectively, measure peak area, the result sees table 4.
Table 4: reproducible test results (n=2)
The result shows: the average content of 5 parts of test samples is 1.22mg/g, and RSD is 1.70%, proves that the repeatability of this test method is good.
9) recovery test (adopting the application of sample absorption method):
Precision takes by weighing 060302 crowd of (known Borneolum Syntheticum content is 1.22mg/g) sample 0.25g, gets 5 parts altogether, the accurate respectively Borneolum Syntheticum reference substance that adds 0.3mg, and the same legal system is equipped with need testing solution, measures total content, calculate recovery rate.The response rate=(measuring in total amount-sample)/pure article amount of adding * 100%.The result sees table 5.
Table 5 Borneolum Syntheticum recovery test result (n=2)
The result shows: the Borneolum Syntheticum average recovery rate is 99.9%, and RSD is 0.85%, and average recovery is good.
10) sample determination:
Get the burn and scald liniment that Rongchang Pharmaceutical (Zibo) Co., Ltd. produces, measure by inventive method, Borneolum Syntheticum content is seen table 6.
Table 6: Borneolum Syntheticum assay result
The result shows: product content is all more than 0.9mg/g, and is relatively stable, proves the quality that this inventive method can the better controlled product.
Claims (4)
1. a Chinese medicine for external application of treating burn and scald is characterized in that by following crude drug formulated: Radix et Rhizoma Thalictri 85～102g, Radix Arnebiae (Radix Lithospermi) 56～69g, Radix Scutellariae 85～102g, Radix Sanguisorbae 56～69g, Radix Et Rhizoma Rhei 56～69g and Borneolum Syntheticum 4～6g.
2. the Chinese medicine for external application of treatment burn and scald according to claim 1 is characterized in that by following crude drug formulated: Radix et Rhizoma Thalictri 93g, Radix Arnebiae (Radix Lithospermi) 62.4g, Radix Scutellariae 93g, Radix Sanguisorbae 62.4g, Radix Et Rhizoma Rhei 62.4g and Borneolum Syntheticum 5g.
3. the method for preparing of the Chinese medicine for external application of the described treatment burn and scald of claim 1 is characterized in that getting Radix et Rhizoma Thalictri, Radix Et Rhizoma Rhei, Radix Arnebiae (Radix Lithospermi), Radix Sanguisorbae and Radix Scutellariae and explodes after 18～36 hours to withered and yellow with the Oleum sesami immersion of 1170～1430g, filters; The Cera Flava that adds 15～25g immediately when temperature is reduced to 55～65 ℃, adds Borneolum Syntheticum; Stirring makes its dissolving, when reducing to room temperature, adds the phenol of 4～5ml; Stir, fill promptly gets.
4. the quality determining method of the Chinese medicine for external application of the described treatment burn and scald of claim 1 is characterized in that comprising the quality testing of following aspect:
(1) thin layer of Radix Et Rhizoma Rhei is differentiated:
Get the Chinese medicine for external application 10ml of treatment burn and scald, with alcohol extraction 3 times, each 10ml, merging ethanol liquid is put evaporate to dryness in the water-bath, and residue adds ethanol 1ml makes its dissolving, as need testing solution; Other gets the chrysophanol reference substance, adds ethyl acetate and processes the solution that every 1ml contains 1mg, as reference substance solution;
According to the check of an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 5～10 μ l, reference substance solution 2～5 μ l; Put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be that 15: 5: 1 petroleum ether, Ethyl formate and formic acid mixtures is developing solvent with mass ratio, launch; Take out, dry, under the ultra-violet lamp of 365nm, inspect; Wherein, the boiling point of petroleum ether is 30～60 ℃;
(2) thin layer of Borneolum Syntheticum is differentiated:
Get the Chinese medicine for external application 10ml of treatment burn and scald, with alcohol extraction 3 times, each 10ml, merging ethanol liquid is put evaporate to dryness in the water-bath, and residue adds ethanol 1ml makes its dissolving, as need testing solution; Other gets the Borneolum Syntheticum reference substance, adds ethanol and processes the solution that every 1ml contains 5mg, as reference substance solution;
According to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography check, draw need testing solution 10 μ l, reference substance solution 2～5 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose; With mass ratio is that 9: 1 petroleum ether and ethyl acetate mixture is developing solvent, launches, and takes out; Dry, spray is with 1wt% vanillin sulfuric acid solution, and hot blast drying to clear spot is inspected; Wherein, the boiling point of petroleum ether is 60～90 ℃;
(3) thin layer of Radix Arnebiae (Radix Lithospermi) is differentiated:
Get the Chinese medicine for external application 20ml of treatment burn and scald, with ethanol extraction 3 times, each 20ml, merging ethanol liquid evaporate to dryness, residue adds ethanol 1ml makes its dissolving, as need testing solution; Other gets Radix Arnebiae (Radix Lithospermi) control medicinal material 1g, adds ethanol 10ml dipping 2 hours, filters, and gets filtrating 1ml as reference substance solution;
Check according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography; Draw need testing solution 10 μ l, reference substance solution 2～5 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be 5: 5: 0.5 with mass ratio: 0.1 cyclohexane extraction, toluene, ethyl acetate and formic acid mixtures are developing solvent; Launch; Take out, dry, inspect;
(4) assay of Borneolum Syntheticum in the Borneolum Syntheticum:
Chromatographic condition and system suitability test: the Rtx-Wax capillary column of 30m * 0.53mm * 1.00 μ m, Polyethylene Glycol PEG-20M is an immobile phase; Flame ionization ditector; Injection port, detector temperature are 210 ℃; 150 ℃ of column temperatures; Post flow 8ml/min; Split sampling, split ratio 9: 1; Theoretical cam curve is calculated by the Borneolum Syntheticum peak should be not less than 6000;
The preparation of inner mark solution: it is an amount of that precision takes by weighing the methyl salicylate reference substance, adds ethyl acetate and process the solution that every 1ml contains 0.8mg, subsequent use;
The preparation of reference substance solution: precision takes by weighing the Borneolum Syntheticum reference substance, adds inner mark solution 1ml, is settled to 10ml with ethyl acetate, processes the solution that every 1ml contains 0.05mg, and is subsequent use;
The preparation of need testing solution: get the Chinese medicine for external application 0.5g of treatment burn and scald, the accurate title, decide, and puts in the 10ml volumetric flask, adds inner mark solution 1ml, is settled to 10ml with ethyl acetate, and mixing filters with 0.45 μ m microporous filter membrane, and is subsequent use;
Algoscopy: accurate respectively reference substance solution and each 1 μ l of need testing solution of drawing, inject gas chromatograph is measured, and promptly gets.
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| CN104189183A (en) * | 2014-08-08 | 2014-12-10 | 赵凡涛 | Traditional Chinese medicinal preparation for treating burn and preparation method thereof |
| CN104688980A (en) * | 2015-03-03 | 2015-06-10 | 山东凤鸣堂医药科技有限公司 | Medicine for treating burns and scalds and trauma and preparation method of medicine |
| CN108226342A (en) * | 2018-01-08 | 2018-06-29 | 佛山市洛克威特科技有限公司 | A kind of assay method of Groomwell root oil |
| CN108303490A (en) * | 2018-01-09 | 2018-07-20 | 上海中医药大学 | A kind of thin-layer identification method of purple dendrobium |
| CN109917041A (en) * | 2019-04-04 | 2019-06-21 | 哈尔滨市康隆药业有限责任公司 | The measuring method of a variety of active ingredients content in xiaoshuan tongluo tablet |
| CN109908241A (en) * | 2018-12-29 | 2019-06-21 | 中国人民解放军总医院 | For treating the plant composition of water and gas hot burn |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104189183A (en) * | 2014-08-08 | 2014-12-10 | 赵凡涛 | Traditional Chinese medicinal preparation for treating burn and preparation method thereof |
| CN104688980A (en) * | 2015-03-03 | 2015-06-10 | 山东凤鸣堂医药科技有限公司 | Medicine for treating burns and scalds and trauma and preparation method of medicine |
| CN108226342A (en) * | 2018-01-08 | 2018-06-29 | 佛山市洛克威特科技有限公司 | A kind of assay method of Groomwell root oil |
| CN108303490A (en) * | 2018-01-09 | 2018-07-20 | 上海中医药大学 | A kind of thin-layer identification method of purple dendrobium |
| CN109908241A (en) * | 2018-12-29 | 2019-06-21 | 中国人民解放军总医院 | For treating the plant composition of water and gas hot burn |
| CN109917041A (en) * | 2019-04-04 | 2019-06-21 | 哈尔滨市康隆药业有限责任公司 | The measuring method of a variety of active ingredients content in xiaoshuan tongluo tablet |
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